Thermogravimetry, diffuse reflectance infrared Fourier transform spectroscopy, and X-ray photoelectron spectroscopy (XPS) were used for the studying of thermally induced structural changes of polyacrylonitrile (PAN) deposited on the surface of SBA-15 type mesoporous silica. Polymer was introduced onto the support by the precipitation polymerization of acrylonitrile in aqueous suspension of SBA-15. Low temperature transformation (to 723 K) of the deposited PAN was analyzed. It was found that at about 523 K, exothermic cyclization of polymer chains to the so-called ladder form of PAN occurred. However, the total cyclization of PAN required higher carbonization temperatures, at which gradual dehydrogenation followed by graphitization was initiated. XPS revealed that the cyclic form of PAN and a relatively large amount of carbonyl species, formed during the carbonization of the PAN/SBA-15 composite at 623 K, were responsible for the high sorption capacity in the methylethyl ketone (MEK) vapor elimination. The efficiency in the MEK adsorption was also influenced by the content of PAN-derived carbon deposited on the SBA-15 surface.Keywords Thermal transformation of polyacrylonitrile Á SBA-15 support Á Thermogravimetry Á X-ray photoelectron spectroscopy Á Diffuse reflectance Fourier transform spectroscopy Á Adsorption of volatile organic compounds